CN106196887A - A kind of method of efficient production High Purity Nitrogen and device thereof and product - Google Patents

A kind of method of efficient production High Purity Nitrogen and device thereof and product Download PDF

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Publication number
CN106196887A
CN106196887A CN201610731674.8A CN201610731674A CN106196887A CN 106196887 A CN106196887 A CN 106196887A CN 201610731674 A CN201610731674 A CN 201610731674A CN 106196887 A CN106196887 A CN 106196887A
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pressure
nitrogen
air
liquid
rectifying column
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CN106196887B (en
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周大荣
俞健
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SHANGHAI QIYUAN GAS DEVELOPMENT Co.,Ltd.
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SHANGHAI QIYUAN AIR SEPARATION TECHNOLOGY DEVELOPMENT Co Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04424—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system without thermally coupled high and low pressure columns, i.e. a so-called split columns
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger

Abstract

A kind of method that the invention provides efficient production High Purity Nitrogen, have employed the device of a kind of efficient production High Purity Nitrogen, in described method: one raw air is separated into oxygen-enriched liquid air and high pressure nitrogen in high-pressure rectification tower, this oxygen-enriched liquid air enters in high-pressure rectification tower condenser/evaporator and flashes to middle pressure oxygen rich air and be transported to middle pressure rectifying column；The most therefrom pressure rectifying column isolates medium pressure nitrogen gas and oxygen-rich liquid, this medium pressure nitrogen gas presses rectifying column condenser/evaporator to be condensed into middle hydraulic fluid nitrogen in entering, in part, hydraulic fluid nitrogen is back to high-pressure rectification tower after liquid nitrogen pump supercharging, highly purified high pressure nitrogen is obtained, its extraction rate reached to 60 75% at high-pressure rectification top of tower；The backflow energy consumption of nitrogen producing craft of oxygen rich air swell refrigeration of the observable index single column of the method unit product reduces about 20 30%, and product safety is reliable, available extensively application, has good market prospect.

Description

A kind of method of efficient production High Purity Nitrogen and device thereof and product
Technical field
The invention belongs to gas generation field, relate to a kind of method carrying out gas separation by low-temperature liquefaction, relate to especially And a kind of method of efficient production High Purity Nitrogen, and the invention still further relates to the device of a kind of efficient production High Purity Nitrogen, and use Described method produces the product prepared.
Background technology
Along with the fast development of the industries such as precision electronic industries, biological medicine, chemical industry, the demand of High Purity Nitrogen is drastically increased Big and require high, the pressure of specific requirement high pure nitrogen is 0.5 ~ 1.2MPa, and nitrogen gas purity 99.9%-99.9999% needs simultaneously Want a small amount of liquid nitrogen (≤5% nitrogen output) for standby.
Prior art a kind of separates air-making and takes the method for pressure nitrogen gas to have employed single column oxygen rich air (waste gas) of backflowing swollen Swollen nitrogen processed, nitrogen pressure, at 0.4-1.2MPa, nitrogen extraction ratio 45-58%, is gas-liquid owing to this technique enters the gas of rectifying column Saturated or band liquid status, the liquid especially into tower is not involved in rectification；Its energy consumption is at 0.26-0.4KWh/NM3N2, The energy consumption of visible the method is higher and pressure is the most up to standard.In prior art, common another kind of preparing pressure nitrogen gas with air separation Method have employed air expansion single column nitrogen, nitrogen pressure at 0.2-0.3 MPa, its energy consumption about 0.23 KWh/NM3N2, because of This, energy consumption is still high and pressure is the most up to standard.In prior art, a kind of method of preparing pressure nitrogen gas with air separation uses Oxygen rich air swell refrigeration (double tower backflows) flow process of evaporation at the bottom of double tower nitrogen, lower pressure column, gained nitrogen pressure is at 0.2- During 0.25MPa, energy consumption is about 0.22 KWh/NM3N2, therefore, the method still can not fully meet the demand of actual production.
In the prior art, Chinese patent CN100581996C discloses the device of a kind of preparing pressure nitrogen gas with air separation And method, this device includes booster expansion turbine, air cooler, main heat exchanger, lower pressure column, is arranged in lower pressure column Boiling device, lower pressure column condenser/evaporator, high-pressure tower, high-pressure tower condenser/evaporator and subcooler；The method by raw air by leading Heat exchanger cooling enters booster expansion turbine, after expansion refrigeration, enters lower pressure column rectification and separates, obtain high-purity at low pressure tower top The pressure nitrogen gas of degree is as output of products；Part material air enters high-pressure tower rectification after entering main heat exchanger cooling and separates, at height Pressure tower top obtains high pressure nitrogen can be as output of products；The extraction ratio of the nitrogen that the method prepares is up to 78-86%, nitrogen pressure At 0.2-0.3MPa, its energy consumption is at 0.18-0.26 KWh/NM3N2。
As can be seen here, prior art there is no the high efficacious prescriptions that a kind of production can reach the High Purity Nitrogen of These parameters Method, therefore, develops a kind of method isolating High Purity Nitrogen from air, and guarantee the pressure of gained nitrogen be 0.5 ~ 1.2MPa, nitrogen gas purity 99.9%-99.9999%, and there is a small amount of liquid nitrogen (≤5% nitrogen output), become current Chemical R & D One of study hotspot of personnel.
Summary of the invention
It is contemplated that overcome many disadvantages present in above-mentioned prior art, and one is provided to divide from air efficiently The method separating out High Purity Nitrogen, meets the demand using High Purity Nitrogen in the field such as precision electronic industries, biological medicine, and guarantees gained The pressure of nitrogen is 0.5 ~ 1.2MPa, nitrogen gas purity 99.9%-99.9999%, and there is a small amount of liquid nitrogen；It is provided simultaneously with extraction ratio The feature high, energy consumption is low.
Therefore, a first aspect of the present invention provides a kind of method of efficient production High Purity Nitrogen, comprises the steps:
The input dried air of purification, is divided into two strands of raw airs:
Wherein one raw air is directly entered main heat exchanger E1, and is cooled to saturation in main heat exchanger E1, produces full And air, then saturated air is delivered to high-pressure rectification tower C1 tower reactor；
Wherein another gang of raw air entrance supercharger Z01 carries out supercharging, is then cooled to room temperature through air cooler E3, then Enter in described main heat exchanger E1 and cool down further, then extract out from the middle part of described main heat exchanger E1, enter turbo-expander ET01 expands, and finally enters the middle and lower part of middle pressure rectifying column C2；
Described high-pressure rectification tower C1 is used for isolating oxygen-enriched liquid air and high pressure nitrogen；
Wherein, described oxygen-enriched liquid air is extracted out bottom described high-pressure rectification tower C1, supercool through subcooler E2, throttling after, enter height Pressure rectifying column condenser/evaporator K1 in flash to gaseous state and export in pressure oxygen rich air, medium pressure oxygen rich air be transported further to Middle pressure rectifying column C2 tower reactor；
Wherein, described high pressure nitrogen is extracted out from described high-pressure rectification tower C1 tower top, and is divided into two strands: first strand of high pressure nitrogen and enters Enter and described high-pressure rectification tower condenser/evaporator K1 is condensed into liquid nitrogen, and mix with the supercharging liquid nitrogen of liquid nitrogen pump P01 output, To liquid nitrogen reflux liquid, described liquid nitrogen reflux liquid is back to the tower top of described high-pressure rectification tower C1；Warp after second strand of high pressure nitrogen is first After described main heat exchanger E1, described air cooler E3 re-heat, as high pure nitrogen output of products；
Medium pressure rectifying column C2 is used for isolating medium pressure nitrogen gas and oxygen-rich liquid；
Wherein, medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, and presses rectifying column condenser/evaporator K2 in entrance, It is condensed into middle hydraulic fluid nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column C2 tower Top, as the backflow pressing rectifying column in this；In second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump P01, after this liquid nitrogen pump supercharging Export described supercharging liquid nitrogen；
Wherein, described oxygen-rich liquid is extracted out bottom medium pressure rectifying column C2, after, throttling supercool through subcooler E2, enters described Middle pressure rectifying column condenser/evaporator K2, flashes to oxygen rich air, through described subcooler E2, described main heat exchanger after described oxygen rich air is first After E1 re-heat, export as oxygen rich air side-product.
Preferably, in the above-mentioned methods, described wherein one raw air is directly entered main heat exchanger E1, and at main heat exchange Device E1 is cooled to saturation, produces the saturated air of-150 ~-170 DEG C, then described saturated air is delivered to high pressure essence Evaporate tower C1 tower reactor.
Preferably, in the above-mentioned methods, described another strand of raw air enter supercharger Z01 be pressurized to 0.80 ~ 1.25MPa, is then cooled to room temperature through air cooler E3, subsequently enters in described main heat exchanger E1 and is cooled further to-120 ~-140 DEG C, then extract out from the middle part of described main heat exchanger E1, enter turbo-expander ET01 and be expanded to 0.18 ~ 0.25MPa, Rear entrance is pressed the middle and lower part of rectifying column C2.
Preferably, in the above-mentioned methods, described oxygen-enriched liquid air is extracted out bottom described high-pressure rectification tower C1, through subcooler E2 Supercool, throttling, to after 0.20 ~ 0.30MPa, enters back in high-pressure rectification tower condenser/evaporator K1.
Preferably, in the above-mentioned methods, described oxygen-rich liquid is extracted out bottom medium pressure rectifying column C2, through subcooler E2 mistake Cold, throttling, to after 0.02 ~ 0.04MPa, enters back in medium pressure rectifying column condenser/evaporator K2.
Preferably, in the above-mentioned methods, in described second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump P01, is increased by this liquid nitrogen pump Described supercharging liquid nitrogen is exported after being depressed into 0.85 ~ 1.25MPa.
Preferably, in the above-mentioned methods, the operation pressure of described high-pressure rectification tower C1 is 0.9 ~ 1.3MPa, medium pressure essence The operation pressure evaporating tower C2 is 0.3 ~ 0.5MPa.
It is further preferred that the device of this efficient production High Purity Nitrogen can be improved, particularly as follows: by middle pressure rectifying column C2 Medium pressure nitrogen gas outlet branches be two pipelines, wherein a pipeline is connected in medium pressure rectifying column condenser/evaporator K2 Pressure nitrogen inlet, wherein another pipeline is connected to the medium pressure nitrogen gas entrance of liquid nitrogen storage tank G01；Correspondingly, middle pressure rectifying column is cold Liquid nitrogen import and the liquid nitrogen entrance of liquid nitrogen storage tank G01 of rectifying column C2 is pressed in the liquid nitrogen outlet of solidifying vaporizer K2 in connecting respectively, and The liquid nitrogen outlet of described liquid nitrogen storage tank G01 is respectively connecting to liquid nitrogen import and the liquid nitrogen export pipeline of high-pressure rectification tower C1, described Liquid nitrogen export pipeline is used for exporting high-purity liquid nitrogen product.Therefore, the method for described efficient production High Purity Nitrogen also includes producing high-purity The step of liquid nitrogen product:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, is divided into two parts, and a portion medium pressure nitrogen gas flows into Liquid nitrogen storage tank G01；Wherein another part medium pressure nitrogen gas enters medium pressure rectifying column condenser/evaporator K2, is condensed into middle hydraulic fluid Nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column C2 tower top, as pressure essence in this Evaporate the backflow of tower；In second strand, hydraulic fluid nitrogen flows into described liquid nitrogen storage tank G01；
The liquid nitrogen liquid storage flowed out from described liquid nitrogen storage tank G01, splits into two parts, and Part I liquid nitrogen liquid storage enters described liquid nitrogen Pump P01, is exported described supercharging liquid nitrogen by after this liquid nitrogen pump supercharging；Part II liquid nitrogen liquid storage, directly as high-purity liquid nitrogen product Output；
Wherein, described High Purity Nitrogen includes described high pure nitrogen product and described high-purity liquid nitrogen product.
It is further preferred that in the above-mentioned methods, recirculated cooling water is used to be situated between as the cooling of described air cooler E3 Matter.
A second aspect of the present invention, it is provided that the device of a kind of efficient production High Purity Nitrogen, is used for implementing said method, described Device includes following equipment:
Turbo-expander ET01 and coupled supercharger Z01, air cooler E3, main heat exchanger E1, high-pressure rectification tower C1, High-pressure rectification tower condenser/evaporator K1, subcooler E2, middle pressure rectifying column C2, middle pressure rectifying column condenser/evaporator K2, liquid nitrogen pump P01, choke valve V301, choke valve V501, if other valve and trunk pipeline, be used for connecting above each equipment；Further, above-mentioned respectively set Annexation between Bei is as follows:
Supercharger Z01 import connects raw air branch road one, and supercharger Z01 outlet connects the raw air of air cooler E3 and enters Mouthful, the outlet of the raw air of air cooler E3 connects the first raw air import of main heat exchanger E1, the of main heat exchanger E1 One raw air outlet connects turbo-expander ET01 entrance, and turbo-expander ET01 outlet is connected to the former of middle pressure rectifying column C2 Material air intlet；
The second raw air import of main heat exchanger E1 connects raw air branch road two, and second raw air of main heat exchanger E1 goes out Mouth is connected to the raw air import of high-pressure rectification tower C1；
The oxygen-enriched liquid air outlet of high-pressure rectification tower C1 is connected to the high-pressure oxygen-enriched liquid air import of subcooler E2, the high pressure of subcooler E2 Oxygen-enriched liquid air outlet is connected to the oxygen-enriched liquid air import of high-pressure rectification tower condenser/evaporator K1 through choke valve V301；High-pressure rectification tower The middle pressure oxygen rich air outlet of condenser/evaporator K1 is connected to the oxygen rich air import of middle pressure rectifying column C2；
The high pressure nitrogen outlet branches of high-pressure rectification tower C1 is two pipelines, and wherein a pipeline connects the condensation steaming of high-pressure rectification tower Sending out the high pressure nitrogen import of device K1, wherein another pipeline connects the high pressure nitrogen import of main heat exchanger E1；High-pressure rectification tower is cold The liquid nitrogen outlet of solidifying vaporizer K1 connects outlet and the liquid nitrogen import of high-pressure rectification tower C1 of liquid nitrogen pump P01 respectively；
The oxygen-rich liquid outlet of middle pressure rectifying column C2 connects the middle pressure oxygen-rich liquid import of subcooler E2, the middle pressure oxygen-rich liquid of subcooler E2 Export the oxygen-rich liquid import pressing rectifying column condenser/evaporator K2 in choke valve V501 connects, middle pressure rectifying column condenser/evaporator K2 Oxygen rich air outlet connect the oxygen rich air import of subcooler E2, the oxygen rich air outlet of subcooler E2 is connected to the richness of main heat exchanger E1 Oxygen inlet, the oxygen rich air outlet of main heat exchanger E1 connects oxygen rich air side-product export pipeline；
The medium pressure nitrogen gas outlet of middle pressure rectifying column C2 is connected to the medium pressure nitrogen gas import of middle pressure rectifying column condenser/evaporator K2, middle pressure The liquid nitrogen outlet of rectifying column condenser/evaporator K2 presses the liquid nitrogen import of rectifying column C2 and the liquid nitrogen of liquid nitrogen pump P01 to enter in connecting respectively Mouthful；The liquid nitrogen outlet of liquid nitrogen pump P01 is connected to the liquid nitrogen import of high-pressure rectification tower C1；
The high pressure nitrogen outlet of main heat exchanger E1 connects the high pressure nitrogen import of air cooler E3, the high pressure of air cooler E3 Nitrogen outlet connects high pressure nitrogen export pipeline, is used for exporting high pure nitrogen product.
A third aspect of the present invention, it is provided that the high pure nitrogen that a kind of method described in first aspect present invention prepares produces Product, the output pressure of described high pure nitrogen product is 0.5 ~ 1.2MPa, wherein N2Purity is 99.9% ~ 99.9999%, and energy consumption is about 0.2-0.23 KWh/NM3N2.Visible, obtained High Purity Nitrogen has reached relevant national standard.
Compared with prior art, the invention have the advantages that
(1) present invention can realize the extraction rate reached of High Purity Nitrogen to 60-75%；The observable index list of the method for the invention unit product The backflow energy consumption of nitrogen producing craft of oxygen rich air swell refrigeration of tower reduces about 20-30%；
(2) output pressure of the high pure nitrogen product obtained reaches 0.5 ~ 1.2MPa, N2High purity 99.9% ~ 99.9999%；
(3) High Purity Nitrogen product form is various, and the High Purity Nitrogen product of production can be gas, it is possible to for part liquid nitrogen product, can quilt It is delivered to liquid storage groove storage further；
(4) method of efficient production High Purity Nitrogen provided by the present invention, with air as raw material, economical and practical, and product safety is reliable, The available extensively application of the method, has good market prospect.
Accompanying drawing explanation
Fig. 1 is the technological process method schematic diagram of the device efficiently producing High Purity Nitrogen described in embodiment 1；
Wherein: 101 is the dried air of the purification in main line, 102,201 it is respectively one raw air, another strand of raw material sky Gas (the dried air of purification in branch road), 103 is the saturated air from main heat exchanger E1 output, and 202 is the sky after supercharging Gas, 203 is the air before expanding, and 204 is the air after expanding；401,402,405,406 is high pressure nitrogen, and 403 is liquid nitrogen, 404 is liquid nitrogen reflux liquid, and 416 is supercharging liquid nitrogen, and 407,408 is medium pressure nitrogen gas, and 409,410,411,412,414 is middle hydraulic fluid Nitrogen, 301,302,303 is oxygen-enriched liquid air, and 304 is middle pressure oxygen rich air, and 501,502,503 is to extract out bottom middle pressure rectifying column C2 Oxygen-rich liquid, 504 is the oxygen rich air after evaporation, and 505 is oxygen rich air, and 506 is oxygen rich air side-product, and E1 is main heat exchanger, and E2 was Cooler, E3 is air cooler, and K1 is high-pressure rectification tower condenser/evaporator, and K2 is middle pressure rectifying column condenser/evaporator, and C1 is high Pressure rectifying column, C2 is middle pressure rectifying column, and ET01 is turbo-expander, and Z01 is the supercharger connecting turbo-expander, V301, V501 is choke valve, and V201, V401, V402, V403, V404 are control valve；
Fig. 2 is the technological process method schematic diagram of the device efficiently producing High Purity Nitrogen described in embodiment 2；
Wherein: 101 is the dried air of the purification in main line, 102,201 it is respectively one raw air, another strand of raw material sky Gas (the dried air of purification in branch road), 103 is the saturated air from main heat exchanger E1 output, and 202 is the sky after supercharging Gas, 203 is the air before expanding, and 204 is the air after expanding；401,402,405,406 is high pressure nitrogen, and 403 is liquid nitrogen, 404 is liquid nitrogen reflux liquid, and 416 is supercharging liquid nitrogen, and 407,408,413 is medium pressure nitrogen gas, and 409,410,411,412,414,415 are Middle hydraulic fluid nitrogen, 301,302,303 is oxygen-enriched liquid air, and 304 is middle pressure oxygen rich air, and 501,502,503 is bottom middle pressure rectifying column C2 The oxygen-rich liquid extracted out, 504 is the oxygen rich air after evaporation, and 505 is oxygen rich air, and 506 is oxygen rich air side-product, and E1 is main heat exchanger, E2 is subcooler, and E3 is air cooler, and K1 is high-pressure rectification tower condenser/evaporator, and K2 is middle pressure rectifying column condenser/evaporator, C1 is high-pressure rectification tower, and C2 is middle pressure rectifying column, and ET01 is turbo-expander, and Z01 is the supercharger connecting turbo-expander, G01 is liquid nitrogen storage tank, and V301, V501 are choke valve, and V201, V401, V402, V403, V404, V506 are control valve.
Detailed description of the invention
A first aspect of the present invention, it is provided that a kind of method of efficient production High Purity Nitrogen, comprises the steps:
The input dried air of purification, is divided into two strands of raw airs:
Wherein one raw air is directly entered main heat exchanger E1, and is cooled to saturation in main heat exchanger E1, produces full And air, then saturated air is delivered to high-pressure rectification tower C1 tower reactor；
Wherein another gang of raw air entrance supercharger Z01 carries out supercharging, is then cooled to room temperature through air cooler E3, then Enter in described main heat exchanger E1 and cool down further, then extract out from the middle part of described main heat exchanger E1, enter turbo-expander ET01 expands, and finally enters the middle and lower part of middle pressure rectifying column C2；
Described high-pressure rectification tower C1 is used for isolating oxygen-enriched liquid air and high pressure nitrogen；
Wherein, described oxygen-enriched liquid air is extracted out bottom described high-pressure rectification tower C1, supercool through subcooler E2, throttling after, enter height Pressure rectifying column condenser/evaporator K1 in flash to gaseous state and export in pressure oxygen rich air, medium pressure oxygen rich air be transported further to Middle pressure rectifying column C2 tower reactor；
Wherein, described high pressure nitrogen is extracted out from described high-pressure rectification tower C1 tower top, and is divided into two strands: first strand of high pressure nitrogen and enters Enter and described high-pressure rectification tower condenser/evaporator K1 is condensed into liquid nitrogen, and mix with the supercharging liquid nitrogen of liquid nitrogen pump P01 output, To liquid nitrogen reflux liquid, described liquid nitrogen reflux liquid is back to the tower top of described high-pressure rectification tower C1；Warp after second strand of high pressure nitrogen is first After described main heat exchanger E1, described air cooler E3 re-heat, as high pure nitrogen output of products；
Medium pressure rectifying column C2 is used for isolating medium pressure nitrogen gas and oxygen-rich liquid；
Wherein, medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, and presses rectifying column condenser/evaporator K2 in entrance, It is condensed into middle hydraulic fluid nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column C2 tower Top, as the backflow pressing rectifying column in this；In second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump P01, after this liquid nitrogen pump supercharging Export described supercharging liquid nitrogen；
Wherein, described oxygen-rich liquid is extracted out bottom medium pressure rectifying column C2, after, throttling supercool through subcooler E2, enters described Middle pressure rectifying column condenser/evaporator K2, flashes to oxygen rich air, through described subcooler E2, described main heat exchanger after described oxygen rich air is first After E1 re-heat, export as oxygen rich air side-product.
In a preferred embodiment, described wherein one raw air is directly entered main heat exchanger E1, and at main heat exchange Device E1 is cooled to saturation, produces the saturated air of-150 ~-170 DEG C, then described saturated air is delivered to high pressure essence Evaporate tower C1 tower reactor.
In a preferred embodiment, described another strand of raw air enters supercharger Z01 and is pressurized to 0.80 ~ 1.25MPa, Then it is cooled to room temperature through air cooler E3, subsequently enters in described main heat exchanger E1 and be cooled further to-120 ~-140 DEG C, Extract out from the middle part of described main heat exchanger E1 again, enter turbo-expander ET01 and be expanded to 0.18 ~ 0.25MPa, in finally entering The middle and lower part of pressure rectifying column C2.
In a preferred embodiment, described oxygen-enriched liquid air is extracted out bottom described high-pressure rectification tower C1, through subcooler E2 Supercool, throttling, to after 0.20 ~ 0.30MPa, enters back in high-pressure rectification tower condenser/evaporator K1.
In a preferred embodiment, described oxygen-rich liquid is extracted out bottom medium pressure rectifying column C2, through subcooler E2 mistake Cold, throttling, to after 0.02 ~ 0.04MPa, enters back in medium pressure rectifying column condenser/evaporator K2.
In a preferred embodiment, in described second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump P01, by this liquid nitrogen pump supercharging Described supercharging liquid nitrogen is exported to 0.85 ~ 1.25MPa.
In a preferred embodiment, the operation pressure of described high-pressure rectification tower C1 is 0.9 ~ 1.3MPa, medium pressure essence The operation pressure evaporating tower C2 is 0.3 ~ 0.5MPa.
In a further preferred embodiment, said method also include produce high-purity liquid nitrogen product step:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, is divided into two parts, and a portion medium pressure nitrogen gas flows into Liquid nitrogen storage tank G01；Wherein another part medium pressure nitrogen gas enters medium pressure rectifying column condenser/evaporator K2, is condensed into middle hydraulic fluid Nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column C2 tower top, as pressure essence in this Evaporate the backflow of tower；In second strand, hydraulic fluid nitrogen flows into described liquid nitrogen storage tank G01；
The liquid nitrogen liquid storage flowed out from described liquid nitrogen storage tank G01, splits into two parts, and Part I liquid nitrogen liquid storage enters described liquid nitrogen Pump P01, is exported described supercharging liquid nitrogen by after this liquid nitrogen pump supercharging；Part II liquid nitrogen liquid storage, directly as high-purity liquid nitrogen product Output；
Wherein, described High Purity Nitrogen includes described high pure nitrogen product and described high-purity liquid nitrogen product.
In a further preferred embodiment, recirculated cooling water is used to be situated between as the cooling of described air cooler E3 Matter.
A second aspect of the present invention, it is provided that the device of a kind of efficient production High Purity Nitrogen, including following equipment:
Turbo-expander ET01 and coupled supercharger Z01, air cooler E3, main heat exchanger E1, high-pressure rectification tower C1, High-pressure rectification tower condenser/evaporator K1, subcooler E2, middle pressure rectifying column C2, middle pressure rectifying column condenser/evaporator K2, liquid nitrogen pump P01, choke valve V301, choke valve V501, if other valve and trunk pipeline, be used for connecting above each equipment；Further, above-mentioned respectively set Annexation between Bei is as follows:
Supercharger Z01 import connects raw air branch road one, and supercharger Z01 outlet connects the raw air of air cooler E3 and enters Mouthful, the outlet of the raw air of air cooler E3 connects the first raw air import of main heat exchanger E1, the of main heat exchanger E1 One raw air outlet connects turbo-expander ET01 entrance, and turbo-expander ET01 outlet is connected to the former of middle pressure rectifying column C2 Material air intlet；
The second raw air import of main heat exchanger E1 connects raw air branch road two, and second raw air of main heat exchanger E1 goes out Mouth is connected to the raw air import of high-pressure rectification tower C1；
The oxygen-enriched liquid air outlet of high-pressure rectification tower C1 is connected to the high-pressure oxygen-enriched liquid air import of subcooler E2, the high pressure of subcooler E2 Oxygen-enriched liquid air outlet is connected to the oxygen-enriched liquid air import of high-pressure rectification tower condenser/evaporator K1 through choke valve V301；High-pressure rectification tower The middle pressure oxygen rich air outlet of condenser/evaporator K1 is connected to the oxygen rich air import of middle pressure rectifying column C2；
The high pressure nitrogen outlet branches of high-pressure rectification tower C1 is two pipelines, and wherein a pipeline connects the condensation steaming of high-pressure rectification tower Sending out the high pressure nitrogen import of device K1, wherein another pipeline connects the high pressure nitrogen import of main heat exchanger E1；High-pressure rectification tower is cold The liquid nitrogen outlet of solidifying vaporizer K1 connects outlet and the liquid nitrogen import of high-pressure rectification tower C1 of liquid nitrogen pump P01 respectively；
The oxygen-rich liquid outlet of middle pressure rectifying column C2 connects the middle pressure oxygen-rich liquid import of subcooler E2, the middle pressure oxygen-rich liquid of subcooler E2 Export the oxygen-rich liquid import pressing rectifying column condenser/evaporator K2 in choke valve V501 connects, middle pressure rectifying column condenser/evaporator K2 Oxygen rich air outlet connect the oxygen rich air import of subcooler E2, the oxygen rich air outlet of subcooler E2 is connected to the richness of main heat exchanger E1 Oxygen inlet, the oxygen rich air outlet of main heat exchanger E1 connects oxygen rich air side-product export pipeline；
The medium pressure nitrogen gas outlet of middle pressure rectifying column C2 is connected to the medium pressure nitrogen gas import of middle pressure rectifying column condenser/evaporator K2, middle pressure The liquid nitrogen outlet of rectifying column condenser/evaporator K2 presses the liquid nitrogen import of rectifying column C2 and the liquid nitrogen of liquid nitrogen pump P01 to enter in connecting respectively Mouthful；The liquid nitrogen outlet of liquid nitrogen pump P01 is connected to the liquid nitrogen import of high-pressure rectification tower C1；
The high pressure nitrogen outlet of main heat exchanger E1 connects the high pressure nitrogen import of air cooler E3, the high pressure of air cooler E3 Nitrogen outlet connects high pressure nitrogen export pipeline, is used for exporting high pure nitrogen product.
A third aspect of the present invention, it is provided that the high pure nitrogen that a kind of method described in first aspect present invention prepares produces Product, the output pressure of this high pure nitrogen product is 0.5 ~ 1.2MPa, wherein N2Purity is 99.9% ~ 99.9999%.
Below in conjunction with detailed description of the invention, the present invention is further elaborated, but the present invention is not limited to following example. Each step in described method is conventional steps if no special instructions；Described equipment the most all can be from open business Approach obtains.
Embodiment 1
Employing technological process method production high pure nitrogen product as shown in Figure 1:
By dried for purification air 101(7300 NM3/ h, 0.75MPa) it is divided into two strands of raw airs, wherein: one raw material is empty Gas 102(5500 NM3/ h) enter main heat exchanger E1, and in this main heat exchanger E1, it is cooled to saturation, produce-168 DEG C Saturated air 103, is then delivered to high-pressure rectification tower C1 tower reactor (operation pressure 1.1MPa), at this high-pressure rectification by saturated air Tower C1 is separated into oxygen-enriched liquid air 301 and high pressure nitrogen 401；Another gang of raw air 201(1800 NM3/ h) enter supercharger Z01 is pressurized to 0.92MPa, is then cooled to 20 DEG C through air cooler E3, subsequently enter in main heat exchanger E1 further It is cooled to-140 DEG C, then extracts out from the middle part of described main heat exchanger E1, enter turbo-expander ET01 and be expanded to 0.22MPa, After, the air 204 after expansion presses the middle and lower part of rectifying column C2 in entering；
Oxygen-enriched liquid air 301 is extracted out bottom described high-pressure rectification tower C1, supercool through subcooler E2, through choke valve V301 throttling extremely After 0.25MPa, entering and flash to middle pressure oxygen rich air 304 in high-pressure rectification tower condenser/evaporator K1 and export, medium pressure is oxygen-enriched Gas 304 is transported further to middle pressure rectifying column C2 tower reactor；
High pressure nitrogen 401(5500 NM3/ h) extract out from described high-pressure rectification tower C1 tower top, and it is divided into two strands: first strand of high pressure Nitrogen 402(1500 NM3/ h) enter in described high-pressure rectification tower condenser/evaporator K1 and be condensed into liquid nitrogen 403, and and liquid nitrogen pump The supercharging liquid nitrogen 416(1700 NM of P01 output3/ h) mixing, obtain liquid nitrogen reflux liquid 404, described liquid nitrogen reflux liquid 404 refluxes Tower top to described high-pressure rectification tower C1；Through described main heat exchanger E1, described air cooler after second strand of high pressure nitrogen 405 is first After E3 re-heat, as high pure nitrogen product (high pressure nitrogen 406,4000 NM3/ h, 0.7MPa, oxygen content≤3ppm) output；
Air 204 after expansion and middle pressure oxygen rich air 304(3200NM3/ h) operate pressure 0.3MPa at middle pressure rectifying column C2() in Rectification is separated into medium pressure nitrogen gas 407(3650NM3/ h, oxygen content≤3ppm) and oxygen-rich liquid 501；
Medium pressure nitrogen 407 is extracted out from medium pressure rectifying column C2 tower top, and presses rectifying column condenser/evaporator K2, quilt in entrance It is condensed into middle hydraulic fluid nitrogen 409；Medium pressure liquid nitrogen 409 is divided into hydraulic fluid nitrogen 410 in two strands: first strand and returns medium pressure rectification Tower C2 tower top, as the backflow pressing rectifying column in this；Hydraulic fluid nitrogen 411(1730NM in second strand3/ h, 0.21MPa) enter institute State liquid nitrogen pump P01, after being pressurized to 0.9MPa by this liquid nitrogen pump, export described supercharging liquid nitrogen 416；
Described oxygen-rich liquid 501 is extracted out bottom medium pressure rectifying column C2, supercool through subcooler E2, through choke valve V501 throttling extremely After 0.03MPa, enter medium pressure rectifying column condenser/evaporator K2, flash to oxygen rich air 504, warp after described oxygen rich air 504 is first After described subcooler E2, described main heat exchanger E1 re-heat, export as oxygen rich air side-product 506.
Embodiment 2
The technological process method as shown in Figure 2 of employing produces high pure nitrogen product and high-purity liquid nitrogen product:
By dried for purification air 101(7300 NM3/ h, 0.72MPa) it is divided into two strands of raw airs, wherein: one raw material is empty Gas 102(5500 NM3/ h) enter main heat exchanger E1, and in this main heat exchanger E1, it is cooled to saturation, produce-160 DEG C Saturated air 103, is then delivered to high-pressure rectification tower C1 tower reactor (operation pressure 1.2MPa), at this high-pressure rectification by saturated air Tower C1 is separated into oxygen-enriched liquid air 301 and high pressure nitrogen 401；Another gang of raw air 201(1800 NM3/ h) enter supercharger Z01 is pressurized to 1.15MPa, is then cooled to 20 DEG C through air cooler E3, subsequently enter in main heat exchanger E1 further It is cooled to-129 DEG C, then extracts out from the middle part of described main heat exchanger E1, enter turbo-expander ET01 and be expanded to 0.25MPa, After, the air 204 after expansion presses the middle and lower part of rectifying column C2 in entering；
Oxygen-enriched liquid air 301 is extracted out bottom described high-pressure rectification tower C1, supercool through subcooler E2, through choke valve V301 throttling extremely After 0.21MPa, entering and flash to middle pressure oxygen rich air 304 in high-pressure rectification tower condenser/evaporator K1 and export, medium pressure is oxygen-enriched Gas 304 is transported further to middle pressure rectifying column C2 tower reactor；
High pressure nitrogen 401(5500 NM3/ h) extract out from described high-pressure rectification tower C1 tower top, and it is divided into two strands: first strand of high pressure Nitrogen 402(1500 NM3/ h) enter in described high-pressure rectification tower condenser/evaporator K1 and be condensed into liquid nitrogen 403, and and liquid nitrogen pump The supercharging liquid nitrogen 416(1700 NM of P01 output3/ h) mixing, obtain liquid nitrogen reflux liquid 404, described liquid nitrogen reflux liquid 404 refluxes Tower top to described high-pressure rectification tower C1；Through described main heat exchanger E1, described air cooler after second strand of high pressure nitrogen 405 is first After E3 re-heat, as high pure nitrogen product (high pressure nitrogen 406,4000 NM3/ h, 0.8MPa, oxygen content≤3ppm) output；
Air 204 after expansion and middle pressure oxygen rich air 304(3200NM3/ h) operate pressure 0.32MPa at middle pressure rectifying column C2() Middle rectification is separated into medium pressure nitrogen gas 407(3650NM3/ h, oxygen content≤3ppm) and oxygen-rich liquid 501；
Medium pressure nitrogen 407 is extracted out from medium pressure rectifying column C2 tower top, is divided into two parts, a portion medium pressure nitrogen gas 413 flow into liquid nitrogen storage tank G01；Wherein another part medium pressure nitrogen gas 408 enters medium pressure rectifying column condenser/evaporator K2, cold Congeal into middle hydraulic fluid nitrogen 409；Medium pressure liquid nitrogen 409 is divided into hydraulic fluid nitrogen 410 in two strands: first strand and returns medium pressure rectifying column C2 tower top, as the backflow pressing rectifying column in this；Hydraulic fluid nitrogen 411(1730NM in second strand3/ h, 0.23MPa) flow into described Liquid nitrogen storage tank G01；
The liquid nitrogen liquid storage (middle hydraulic fluid nitrogen 414) flowed out from described liquid nitrogen storage tank G01, splits into two parts, and Part I liquid nitrogen stores up Liquid (1700NM3/ h) enter described liquid nitrogen pump P01, export supercharging liquid nitrogen 416 after being pressurized to 1.08MPa by this liquid nitrogen pump；Second Part liquid nitrogen liquid storage (middle hydraulic fluid nitrogen 415,30NM3/ h), directly as high-purity liquid nitrogen output of products；
Described oxygen-rich liquid 501 is extracted out bottom medium pressure rectifying column C2, supercool through subcooler E2, through choke valve V501 throttling extremely After 0.02MPa, enter medium pressure rectifying column condenser/evaporator K2, flash to oxygen rich air 504, warp after described oxygen rich air 504 is first After described subcooler E2, described main heat exchanger E1 re-heat, export as oxygen rich air side-product 506.
Being described in detail the specific embodiment of the present invention above, but it is intended only as example, the present invention does not limit It is formed on particular embodiments described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and Substitute the most all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and Amendment, all should contain within the scope of the invention.

Claims (10)

1. the method for an efficient production High Purity Nitrogen, it is characterised in that comprise the steps:
The input dried air of purification, is divided into two strands of raw airs:
Wherein one raw air is directly entered main heat exchanger (E1), and is cooled to saturation in main heat exchanger (E1), produces Raw saturated air, is then delivered to high-pressure rectification tower (C1) tower reactor by saturated air；
Wherein another burst of raw air entrance supercharger (Z01) carries out supercharging, is then cooled to room temperature through air cooler (E3), Subsequently enter in described main heat exchanger (E1) and cool down further, then extract out from the middle part of described main heat exchanger (E1), enter turbine Decompressor (ET01) expands, and finally enters the middle and lower part of middle pressure rectifying column (C2)；
Described high-pressure rectification tower (C1) is used for isolating oxygen-enriched liquid air and high pressure nitrogen；
Wherein, described oxygen-enriched liquid air from described high-pressure rectification tower (C1) bottom extract out, supercool through subcooler (E2), throttling after, enter Pressing oxygen rich air in entering to flash in high-pressure rectification tower condenser/evaporator (K1) gaseous state and exporting, medium pressure oxygen rich air is by further It is delivered to middle pressure rectifying column (C2) tower reactor；
Wherein, described high pressure nitrogen is extracted out from described high-pressure rectification tower (C1) tower top, and is divided into two strands: first strand of high pressure nitrogen Enter and described high-pressure rectification tower condenser/evaporator (K1) is condensed into liquid nitrogen, and the supercharging liquid nitrogen exported with liquid nitrogen pump (P01) Mixing, obtains liquid nitrogen reflux liquid, and described liquid nitrogen reflux liquid is back to the tower top of described high-pressure rectification tower (C1)；Second burst of elevated pressure nitrogen After gas is first after described main heat exchanger (E1), described air cooler (E3) re-heat, as high pure nitrogen output of products；
Medium pressure rectifying column (C2) is used for isolating medium pressure nitrogen gas and oxygen-rich liquid；
Wherein, medium pressure nitrogen is extracted out from medium pressure rectifying column (C2) tower top, and presses rectifying column condenser/evaporator in entrance (K2), it is condensed into middle hydraulic fluid nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column (C2) tower top, as the backflow pressing rectifying column in this；In second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump (P01), by this liquid nitrogen Described supercharging liquid nitrogen is exported after pump supercharging；
Wherein, described oxygen-rich liquid from medium pressure rectifying column (C2) bottom extract out, supercool through subcooler (E2), throttling after, enter Medium pressure rectifying column condenser/evaporator (K2), flashes to oxygen rich air, described oxygen rich air first after through described subcooler (E2), described After main heat exchanger (E1) re-heat, export as oxygen rich air side-product.
Method the most according to claim 1, it is characterised in that described wherein one raw air is directly entered main heat exchanger (E1), and in main heat exchanger (E1), it is cooled to saturation, produces the saturated air of-150 ~-170 DEG C, then by described full It is delivered to high-pressure rectification tower (C1) tower reactor with air.
Method the most according to claim 1, it is characterised in that described another strand of raw air enters supercharger (Z01) and increase It is depressed into 0.80 ~ 1.25MPa, is then cooled to room temperature through air cooler (E3), subsequently enter in described main heat exchanger (E1) One step is cooled to-120 ~-140 DEG C, then extracts out from the middle part of described main heat exchanger (E1), enters turbo-expander (ET01) and expands To 0.18 ~ 0.25MPa, finally enter the middle and lower part of middle pressure rectifying column (C2).
Method the most according to claim 1, it is characterised in that described oxygen-enriched liquid air is from described high-pressure rectification tower (C1) bottom Extracting out, throttling supercool through subcooler (E2), to after 0.20 ~ 0.30MPa, enters back in high-pressure rectification tower condenser/evaporator (K1).
Method the most according to claim 1, it is characterised in that described oxygen-rich liquid is taken out from medium pressure rectifying column (C2) bottom Going out, throttling supercool through subcooler (E2), to after 0.02 ~ 0.04MPa, enters back into medium pressure rectifying column condenser/evaporator (K2) In.
Method the most according to claim 1, it is characterised in that in described second strand, hydraulic fluid nitrogen enters described liquid nitrogen pump (P01) described supercharging liquid nitrogen is exported after, being pressurized to 0.85 ~ 1.25MPa by this liquid nitrogen pump.
Method the most according to claim 1, it is characterised in that the operation pressure of described high-pressure rectification tower (C1) is 0.9 ~ 1.3MPa, the operation pressure of medium pressure rectifying column (C2) is 0.3 ~ 0.5MPa.
8. according to the method according to any one of claim 1 ~ 7, it is characterised in that also include the step producing high-purity liquid nitrogen product Rapid:
Medium pressure nitrogen is extracted out from medium pressure rectifying column (C2) tower top, is divided into two parts, a portion medium pressure nitrogen air-flow Enter liquid nitrogen storage tank (G01)；Wherein another part medium pressure nitrogen gas enters medium pressure rectifying column condenser/evaporator (K2), is condensed into Middle hydraulic fluid nitrogen；Medium pressure liquid nitrogen is divided into hydraulic fluid nitrogen in two strands: first strand and returns medium pressure rectifying column (C2) tower top, as This presses the backflow of rectifying column；In second strand, hydraulic fluid nitrogen flows into described liquid nitrogen storage tank (G01)；
The liquid nitrogen liquid storage flowed out from described liquid nitrogen storage tank (G01), splits into two parts, and Part I liquid nitrogen liquid storage enters described liquid Nitrogen pump (P01), is exported described supercharging liquid nitrogen by after this liquid nitrogen pump supercharging；Part II liquid nitrogen liquid storage, directly as high-purity liquid nitrogen Output of products；
Wherein, described High Purity Nitrogen includes described high pure nitrogen product and described high-purity liquid nitrogen product.
9. the device of an efficient production High Purity Nitrogen, it is characterised in that include following equipment:
Turbo-expander (ET01) and coupled supercharger (Z01), air cooler (E3), main heat exchanger (E1), high pressure Rectifying column (C1), high-pressure rectification tower condenser/evaporator (K1), subcooler (E2), middle pressure rectifying column (C2), middle pressure rectifying column condense Vaporizer (K2), liquid nitrogen pump (P01), choke valve (V301), choke valve (V501), if other valve and trunk pipeline, it is used for connecting The most each equipment；Further, the annexation between above-mentioned each equipment is as follows:
Supercharger (Z01) import connects raw air branch road one, and supercharger (Z01) outlet connects the raw material of air cooler (E3) Air intlet, the raw air outlet of air cooler (E3) connects the first raw air import of main heat exchanger (E1), and master changes First raw air outlet of hot device (E1) connects turbo-expander (ET01) entrance, and turbo-expander (ET01) outlet is connected to The raw air import of middle pressure rectifying column (C2)；
Second raw air import of main heat exchanger (E1) connects raw air branch road two, and the second raw material of main heat exchanger (E1) is empty Gas outlet is connected to the raw air import of high-pressure rectification tower (C1)；
The oxygen-enriched liquid air outlet of high-pressure rectification tower (C1) is connected to the high-pressure oxygen-enriched liquid air import of subcooler (E2), subcooler (E2) The outlet of high-pressure oxygen-enriched liquid air be connected to the oxygen-enriched liquid air import of high-pressure rectification tower condenser/evaporator (K1) through choke valve (V301)； The middle pressure oxygen rich air outlet of high-pressure rectification tower condenser/evaporator (K1) is connected to the oxygen rich air import of middle pressure rectifying column (C2)；
The high pressure nitrogen outlet branches of high-pressure rectification tower (C1) is two pipelines, and wherein a pipeline connects the condensation of high-pressure rectification tower The high pressure nitrogen import of vaporizer (K1), wherein another pipeline connects the high pressure nitrogen import of main heat exchanger (E1)；High pressure essence The liquid nitrogen of outlet and high-pressure rectification tower (C1) that the liquid nitrogen outlet evaporating tower condenser/evaporator (K1) connects liquid nitrogen pump (P01) respectively enters Mouthful；
The oxygen-rich liquid outlet of middle pressure rectifying column (C2) connects the middle pressure oxygen-rich liquid import of subcooler (E2), the middle pressure of subcooler (E2) The oxygen-rich liquid import of rectifying column condenser/evaporator (K2) is pressed in oxygen-rich liquid outlet in choke valve (V501) connects, and middle pressure rectifying column is cold The oxygen rich air outlet of solidifying vaporizer (K2) connects the oxygen rich air import of subcooler (E2), and the oxygen rich air outlet of subcooler (E2) connects To the oxygen rich air import of main heat exchanger (E1), the oxygen rich air outlet of main heat exchanger (E1) connects oxygen rich air side-product export pipeline；
The medium pressure nitrogen gas outlet of middle pressure rectifying column (C2) is connected to the medium pressure nitrogen gas import of middle pressure rectifying column condenser/evaporator (K2), Liquid nitrogen import and the liquid nitrogen pump of rectifying column (C2) is pressed in the liquid nitrogen outlet of middle pressure rectifying column condenser/evaporator (K2) in connecting respectively (P01) liquid nitrogen import；The liquid nitrogen outlet of liquid nitrogen pump (P01) is connected to the liquid nitrogen import of high-pressure rectification tower (C1)；
The high pressure nitrogen outlet of main heat exchanger (E1) connects the high pressure nitrogen import of air cooler (E3), air cooler (E3) High pressure nitrogen outlet connect high pressure nitrogen export pipeline, be used for exporting high pure nitrogen product.
10. the high pure nitrogen product prepared according to the method according to any one of claim 1 ~ 8, it is characterised in that institute The output pressure stating high pure nitrogen product is 0.5 ~ 1.2MPa, wherein N2Purity is 99.9% ~ 99.9999%.
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Publication number Priority date Publication date Assignee Title
CN107062800A (en) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 The method and its device of a kind of superpure nitrogen dehydrogenation
CN107840315A (en) * 2017-12-21 2018-03-27 南京航空航天大学 Airborne oxygen oxygen generation-nitrogen generation coupling system processed and method with expanding machine
CN113551483A (en) * 2021-07-19 2021-10-26 上海加力气体有限公司 Single-tower rectification waste gas backflow expansion nitrogen making system and nitrogen making machine
CN114777415A (en) * 2022-04-22 2022-07-22 杭州特盈能源技术发展有限公司 Low-energy-consumption double-tower double-supercooling positive flow expansion nitrogen production process

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53106673A (en) * 1977-03-02 1978-09-16 Hitachi Ltd Liquefaction separation method for air
CN1103157A (en) * 1993-09-15 1995-05-31 气体产品与化学公司 Cryogenic air separation process producing elevated pressure nitrogen by pumped liquid nitrogen
CN1107572A (en) * 1993-12-22 1995-08-30 英国氧气集团有限公司 Air separation
US6227005B1 (en) * 2000-03-01 2001-05-08 Air Products And Chemicals, Inc. Process for the production of oxygen and nitrogen
CN101367509A (en) * 2008-10-10 2009-02-18 上海启元空分技术发展有限公司 Apparatus and method for preparing pressure nitrogen gas with air separation
CN101886870A (en) * 2010-06-24 2010-11-17 上海启元科技发展有限公司 Method and device for producing pressure high-purity nitrogen and high-purity oxygen
CN206037585U (en) * 2016-08-26 2017-03-22 上海启元空分技术发展股份有限公司 Device of high pure nitrogen of high -efficient production

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53106673A (en) * 1977-03-02 1978-09-16 Hitachi Ltd Liquefaction separation method for air
CN1103157A (en) * 1993-09-15 1995-05-31 气体产品与化学公司 Cryogenic air separation process producing elevated pressure nitrogen by pumped liquid nitrogen
CN1107572A (en) * 1993-12-22 1995-08-30 英国氧气集团有限公司 Air separation
US6227005B1 (en) * 2000-03-01 2001-05-08 Air Products And Chemicals, Inc. Process for the production of oxygen and nitrogen
CN101367509A (en) * 2008-10-10 2009-02-18 上海启元空分技术发展有限公司 Apparatus and method for preparing pressure nitrogen gas with air separation
CN101886870A (en) * 2010-06-24 2010-11-17 上海启元科技发展有限公司 Method and device for producing pressure high-purity nitrogen and high-purity oxygen
CN206037585U (en) * 2016-08-26 2017-03-22 上海启元空分技术发展股份有限公司 Device of high pure nitrogen of high -efficient production

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107062800A (en) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 The method and its device of a kind of superpure nitrogen dehydrogenation
CN107840315A (en) * 2017-12-21 2018-03-27 南京航空航天大学 Airborne oxygen oxygen generation-nitrogen generation coupling system processed and method with expanding machine
CN113551483A (en) * 2021-07-19 2021-10-26 上海加力气体有限公司 Single-tower rectification waste gas backflow expansion nitrogen making system and nitrogen making machine
CN114777415A (en) * 2022-04-22 2022-07-22 杭州特盈能源技术发展有限公司 Low-energy-consumption double-tower double-supercooling positive flow expansion nitrogen production process
CN114777415B (en) * 2022-04-22 2023-08-15 杭州特盈能源技术发展有限公司 Low-energy-consumption double-tower double-supercooling forward expansion nitrogen production process

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